US3472627A - Method and apparatus for separating number of samples displaced in a tubing of small internal diameter - Google Patents

Method and apparatus for separating number of samples displaced in a tubing of small internal diameter Download PDF

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US3472627A
US3472627A US538632A US3472627DA US3472627A US 3472627 A US3472627 A US 3472627A US 538632 A US538632 A US 538632A US 3472627D A US3472627D A US 3472627DA US 3472627 A US3472627 A US 3472627A
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tubing
medium
samples
internal diameter
small internal
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US538632A
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Jiri Hrdina
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Czech Academy of Sciences CAS
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/84—Preparation of the fraction to be distributed
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/08—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a stream of discrete samples flowing along a tube system, e.g. flow injection analysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/11—Automated chemical analysis
    • Y10T436/117497—Automated chemical analysis with a continuously flowing sample or carrier stream
    • Y10T436/118339—Automated chemical analysis with a continuously flowing sample or carrier stream with formation of a segmented stream

Definitions

  • a first medium to be evaluated such as amino acids, contains absorbed therein a second medium and is led towards an evaluating device in a tubing of small internal diameter passing a reactor.
  • the pressure and/or heat conditions in the tubing within the reactor are adjusted to release the absorbed second medium from the first medium by evaporation or by liquefying to separate segments of the first medium before reaching the evaluating device.
  • This invention relates to a method and to an apparatus for separating samples of a medium delivered through a tubing of small internal diameter for analyzing, dispensing or the like in an accordingly operating device.
  • the sample to be analyzed is according to one embodiment pumped by a pump into a tubing of small internal diameter and the individual samples in the tubing are separated by air bubbles introduced into said tubing by the pumping action of another pump so that air divides the fluid stream into a segmented fluid stream composed of alternate segments of liquid and air.
  • a second medium capable to be adsorbed in the displaced first medium is used for separation of samples.
  • the second medium is according to this invention caused to be released from said first medium during its passage through a tubing, creating therein alternate segments of samples of the first medium and segments of the second medium which prevent or at least substantially reduce mixing of different segments of samples of the first medium.
  • tubing of small internal diameter indicates a tubing which is capable 3,472,627 Patented Oct. 14, 1969 to retain intact bubbles or balls of the second medium separating samples of the first medium in the course of displacement of the media.
  • the upper limit of the internal diameter of such a tubing is up to about one eighth of an inch.
  • liquid samples which had to be analyzed have been deliberately deaerated in order to prevent any creation of air bubbles which are segregated particularly at parts of the tubing maintained at elevated temperatures.
  • the treated samples of a fluidal medium to be evaluated and containing absorbed air or some other inert gas are not deaerated, and bubbles of air or gas are released in said tubing when the temperature is raised or the pressure reduced so that the stream of liquid is divided into a number of segments separated by air or gas bubbles.
  • gaseous samples can be separated by balls or bubbles of the second medium which liquefies in case pressure is increased or temperature is reduced.
  • FIG. 1 of the accompanying drawings illustrates the method of the present invention in its simplest embodiment applying a gaseous medium for separation of samples of a liquid medium using heat for the release of gas bubbles.
  • FIG. 2 is an alternative arrangement using in addition reduced pressure to release gas bubbles
  • FIG. 3 is a similar arrangement
  • FIG. 4 shows a pressure reducing valve used for this urpose.
  • FIG. 5 shows a space of reduced pressure connected to the outlet of the tubing
  • FIG. 6 shows the introduction of an evaluating reagent to the outlet of a chromatographic column.
  • a liquid having air or inert gas absorbed is pumped by the pump 3 through the tubing 4 of small internal diameter, the part 1 of said tubing which is immersed in a bath 2 contained in a reactor vessel heated to a temperature at which bubbles of air or gas absorbed in the liquid are released.
  • the thus separated parts of the liquid are displaced by Way of an outlet tubing 6 to an evaluating device 5.
  • the desorption eflect of the bath is increased by placing the pump 3 below the part 1 of the tubing, thus creating reduced pressure at the input to part 1 of the tubing with respect to the pressure at the outlet of the pump 3 due to the hydrostatic elfect.
  • said reduced pressure between the input and output of part 1 of the tubing is achieved by placing the outlet 7 of the tubing 7 behind the evaluating device 5 deeper than the part 1 of the tubing.
  • a reduction in pressure causing desorption of gas bubbles is caused by a pressure reducing valve 8 in tubing 4 behind the pump 3 whereas in front of the pump 3 conditions prevail at which desorption does not take place.
  • the outlet tubing 7 behind the evaluating device 5 is connected to a space 9 wherein reduced pressure is maintained.
  • FIG. 6 shows schematically the application of the object of this invention in connection with a chromatographic analyzer of a liquid.
  • the liquid to be analyzed for instance a mixture of amino acids is pumped by the pump 3 to the chromatographic column 11 containing reagents which cause the difierent phases of the mixture to be displaced in the chromatographic column 11 at different rates.
  • the evaluating reagent for example ninhydrin is added to the outlet conduit of the chromatographic column 11 by means of the pump 12 to the junction 10.
  • the separated amino acids together with the evaluating reagent proceed in tubing 4 to part 1 of the tubing immersed in the bath 2, where bubbles are released; these bubbles divide the up to this moment continuous stream of liquid into a number of segments and prevent in the course of the subsequent passage any mixing of the different phases of the liquid separated in the chromatographic column 11.
  • the thus separated phases are evaluated in the evaluation device 5.
  • the part 1 of tubing 4 Where the desorption of bubbles takes place, is arranged as close as possible to the outlet of the chromatographic column 11 in order to reduce to the possibly highest degree any decrease of concentration gradients in the liquid leaving the chromatographic column 11.
  • the method according to this invention can be applied in other cases, where a number of samples have to be in succession analyzed, for instance difierent samples of urea or blood or for continuous checking of certain conditions in the course of some operation.
  • gaseous media can be treated in a similar manner by releasing for instance in part 1 of the tubing 4 balls of water which were prior evaporated and which separate the different samples of the gaseous medium.
  • the bath 2 has to operate at a reduced temperature or at an increased pressure.
  • a rather important contribution of this invention is the omission of the deaeration of liquids prior to their analyzing. Up to the present the formation of bubbles in the course of heating a liquid which had to be performed prior to its analysis has been rather troublesome and the removal of air absorbed in the liquid generally not sufficiently effective. According to this invention the desorption of gases which particularly takes place in the course of heating of the analyzed liquid is utilized for separating successive samples, so that the up to now troublesome operation rendering a rather poor effect is not required anymore.
  • the method of segmentizing samples of a first fluid medium to be evaluated comprising the steps of absorbing a second fluid medium in the first fluid medium, passing the thus combined fluid media through a tubing of small internal diameter, a portion of the tubing being immersed in a heated reactor, and selectively adjusting at least one of the pressure and the heat conditions existing in the portion of the tubing within the reactor to release the second medium from the first medium, whereby the second medium forms separating segments between resulting segments of the first medium, and the thus separated segments may be passed into the evaluating device.
  • a device to separate samples of a first fiuidal medium, containing an absorbed second fiuidal medium for evaluating in an evaluating device comprising in combination a source for said first medium containing an absorbed second medium; pumping means and an adjoining tubing of small internal diameter carrying said media through a heat reactor into said evaluating device; an exit tubing leading from said evaluating device; and means to selectively adjust at least one of the pressure and heat conditions in the tubing within the reactor to release the second medium from the first medium whereby the second medium forms separating segments between resulting segments of the first medium, and the thus separated segments may be passed to an evaluating device.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Sampling And Sample Adjustment (AREA)

Description

3,472,627 METHOD AND APPARATUS FOR SEPARATING NUMBER OF SAMPLES Oct. 14. 1969 J. HRDINA DISPLACED IN A TUBING OF SMALL INTERNAL DIAMETER Filed March 30, 1966 '2 Sheets-Sheet l FIG. 8
INVENTOR.
Oct. 14,1969 J. HRDINA $472,627
METHOD AND APPARATUS FOR SEPARATING NUMBER OF SAMPLES DISPLACED IN A TUBING OF SMALL INTERNAL DIAMETER Filed March 50, 1966 2 Sheets-Sheet 2 I NVEXTOR.
J [RI HR United States Patent US. Cl. 23-230 6 Claims ABSTRACT OF THE DISCLOSURE A first medium to be evaluated, such as amino acids, contains absorbed therein a second medium and is led towards an evaluating device in a tubing of small internal diameter passing a reactor. The pressure and/or heat conditions in the tubing within the reactor are adjusted to release the absorbed second medium from the first medium by evaporation or by liquefying to separate segments of the first medium before reaching the evaluating device.
This invention relates to a method and to an apparatus for separating samples of a medium delivered through a tubing of small internal diameter for analyzing, dispensing or the like in an accordingly operating device.
'It is frequently required in laboratory practice to separate a number of samples of some liquid or gaseous medium conveyed in a tubing of small internal diameter in order to analyze or the like each of said samples separately without running the risk that the subsequently operated on samples contaminate one another or even become mixed.
A method and an apparatus serving this purpose are described in the US. Patents Nos. 2,797,149, 2,879,141 and 3,047,367 permitting a number of successive analyses to be made in a continuous manner. The sample to be analyzed is according to one embodiment pumped by a pump into a tubing of small internal diameter and the individual samples in the tubing are separated by air bubbles introduced into said tubing by the pumping action of another pump so that air divides the fluid stream into a segmented fluid stream composed of alternate segments of liquid and air. In the course of travel of this segmented fluid stream through the tubing the segments of air displace liquid from the internal surface of the tubing so as to prevent or substantially reduce the mixing of samples with each other and hence prevent the contamination of one sample by another in the course of operation of the apparatus analyzing subsequently a series of separated samples.
Alternately another liquid immiscible with the analyzed samples is intermittently introduced into said tubing with a similar eifect as previously described.
It is an object of this invention to simplify the separation of the different samples of a medium displaced in a tubing of small internal diameter.
In accordance with this invention a second medium capable to be adsorbed in the displaced first medium is used for separation of samples. The second medium is according to this invention caused to be released from said first medium during its passage through a tubing, creating therein alternate segments of samples of the first medium and segments of the second medium which prevent or at least substantially reduce mixing of different segments of samples of the first medium.
In this specification the expression tubing of small internal diameter indicates a tubing which is capable 3,472,627 Patented Oct. 14, 1969 to retain intact bubbles or balls of the second medium separating samples of the first medium in the course of displacement of the media. In practice the upper limit of the internal diameter of such a tubing is up to about one eighth of an inch.
Up to the present, liquid samples which had to be analyzed, have been deliberately deaerated in order to prevent any creation of air bubbles which are segregated particularly at parts of the tubing maintained at elevated temperatures. Contrary thereto according to this invention the treated samples of a fluidal medium to be evaluated and containing absorbed air or some other inert gas are not deaerated, and bubbles of air or gas are released in said tubing when the temperature is raised or the pressure reduced so that the stream of liquid is divided into a number of segments separated by air or gas bubbles. in a similar way gaseous samples can be separated by balls or bubbles of the second medium which liquefies in case pressure is increased or temperature is reduced.
FIG. 1 of the accompanying drawings illustrates the method of the present invention in its simplest embodiment applying a gaseous medium for separation of samples of a liquid medium using heat for the release of gas bubbles.
FIG. 2 is an alternative arrangement using in addition reduced pressure to release gas bubbles,
FIG. 3 is a similar arrangement,
FIG. 4 shows a pressure reducing valve used for this urpose.
FIG. 5 shows a space of reduced pressure connected to the outlet of the tubing; and
FIG. 6 shows the introduction of an evaluating reagent to the outlet of a chromatographic column.
According to FIG. 1 a liquid having air or inert gas absorbed is pumped by the pump 3 through the tubing 4 of small internal diameter, the part 1 of said tubing which is immersed in a bath 2 contained in a reactor vessel heated to a temperature at which bubbles of air or gas absorbed in the liquid are released. The thus separated parts of the liquid are displaced by Way of an outlet tubing 6 to an evaluating device 5.
According to FIG. 2 the desorption eflect of the bath is increased by placing the pump 3 below the part 1 of the tubing, thus creating reduced pressure at the input to part 1 of the tubing with respect to the pressure at the outlet of the pump 3 due to the hydrostatic elfect.
According to FIG. 3 said reduced pressure between the input and output of part 1 of the tubing is achieved by placing the outlet 7 of the tubing 7 behind the evaluating device 5 deeper than the part 1 of the tubing.
According to FIG. 4 a reduction in pressure causing desorption of gas bubbles is caused by a pressure reducing valve 8 in tubing 4 behind the pump 3 whereas in front of the pump 3 conditions prevail at which desorption does not take place.
According to FIG. 5 the outlet tubing 7 behind the evaluating device 5 is connected to a space 9 wherein reduced pressure is maintained.
FIG. 6 shows schematically the application of the object of this invention in connection with a chromatographic analyzer of a liquid. The liquid to be analyzed, for instance a mixture of amino acids is pumped by the pump 3 to the chromatographic column 11 containing reagents which cause the difierent phases of the mixture to be displaced in the chromatographic column 11 at different rates. The evaluating reagent, for example ninhydrin is added to the outlet conduit of the chromatographic column 11 by means of the pump 12 to the junction 10. The separated amino acids together with the evaluating reagent proceed in tubing 4 to part 1 of the tubing immersed in the bath 2, where bubbles are released; these bubbles divide the up to this moment continuous stream of liquid into a number of segments and prevent in the course of the subsequent passage any mixing of the different phases of the liquid separated in the chromatographic column 11. The thus separated phases are evaluated in the evaluation device 5.
It is understood that the part 1 of tubing 4, Where the desorption of bubbles takes place, is arranged as close as possible to the outlet of the chromatographic column 11 in order to reduce to the possibly highest degree any decrease of concentration gradients in the liquid leaving the chromatographic column 11. In a similar way the method according to this invention can be applied in other cases, where a number of samples have to be in succession analyzed, for instance difierent samples of urea or blood or for continuous checking of certain conditions in the course of some operation.
As has been already stated, gaseous media can be treated in a similar manner by releasing for instance in part 1 of the tubing 4 balls of water which were prior evaporated and which separate the different samples of the gaseous medium. In that case the bath 2 has to operate at a reduced temperature or at an increased pressure.
A rather important contribution of this invention is the omission of the deaeration of liquids prior to their analyzing. Up to the present the formation of bubbles in the course of heating a liquid which had to be performed prior to its analysis has been rather troublesome and the removal of air absorbed in the liquid generally not sufficiently effective. According to this invention the desorption of gases which particularly takes place in the course of heating of the analyzed liquid is utilized for separating successive samples, so that the up to now troublesome operation rendering a rather poor effect is not required anymore.
I claim:
1. The method of segmentizing samples of a first fluid medium to be evaluated, comprising the steps of absorbing a second fluid medium in the first fluid medium, passing the thus combined fluid media through a tubing of small internal diameter, a portion of the tubing being immersed in a heated reactor, and selectively adjusting at least one of the pressure and the heat conditions existing in the portion of the tubing within the reactor to release the second medium from the first medium, whereby the second medium forms separating segments between resulting segments of the first medium, and the thus separated segments may be passed into the evaluating device.
2. The method according to claim 1 wherein the second medium is released in gaseous form from the first medium by increase of the heat.
3. The method according to claim 1 wherein the second medium is-released in gaseous form from the first medium by reduction of pressure.
4. The method according to claim 1 wherein the second medium is released in liquefied form from the first medium by reduction of heat.
5. The method according to claim 1 wherein the second medium is released in liquefied form from the first medium by increase of pressure.
6. In a device to separate samples of a first fiuidal medium, containing an absorbed second fiuidal medium for evaluating in an evaluating device, the improvement comprising in combination a source for said first medium containing an absorbed second medium; pumping means and an adjoining tubing of small internal diameter carrying said media through a heat reactor into said evaluating device; an exit tubing leading from said evaluating device; and means to selectively adjust at least one of the pressure and heat conditions in the tubing within the reactor to release the second medium from the first medium whereby the second medium forms separating segments between resulting segments of the first medium, and the thus separated segments may be passed to an evaluating device.
References Cited UNITED STATES PATENTS 2,946,665 7/1960 Skeggs 23-230 3,047,367 7/1962 Kessler 23-230 3,097,927 7/1963 Skeggs 23-230 OTHER REFERENCES Hawk, Oser & Summerson, Practical Physiological Chemistry, 13th edn. McGraw-Hill, QP 514 H4, 1954. Copy in Gp. 170, pp. 129, 130, 892 and 893 relied on.
MORRIS O. WOLK, Primary Examiner R. M. REESE, Assistant Examiner US. Cl. X.R.
US538632A 1965-04-07 1966-03-30 Method and apparatus for separating number of samples displaced in a tubing of small internal diameter Expired - Lifetime US3472627A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3918907A (en) * 1973-10-29 1975-11-11 Beckman Instruments Inc Micro automatic amino acid analysis process and system
WO1982000773A1 (en) * 1980-09-02 1982-03-18 Chemical Co Dow Liquid chromatographic method and apparatus with hollow fiber device for post-column derivatization
EP2438938A1 (en) * 2010-10-11 2012-04-11 PharmaSens AG Syringe type pump
CN103619377A (en) * 2011-04-05 2014-03-05 法玛森斯股份公司 Dermally affixed device for intravenous access

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2240176B (en) * 1987-03-06 1991-12-04 Extrel Corp Introduction of effluent into mass spectrometers and other gas-phase or particle detectors

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2946665A (en) * 1956-09-26 1960-07-26 Technicon Instr Method and means for the determination of carbon dioxide in biological fluids
US3047367A (en) * 1959-12-01 1962-07-31 Technicon Instr Automatic analysis with fluid segmentation
US3097927A (en) * 1959-07-21 1963-07-16 Technicon Instr Chromatography analysis apparatus and method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2946665A (en) * 1956-09-26 1960-07-26 Technicon Instr Method and means for the determination of carbon dioxide in biological fluids
US3097927A (en) * 1959-07-21 1963-07-16 Technicon Instr Chromatography analysis apparatus and method
US3047367A (en) * 1959-12-01 1962-07-31 Technicon Instr Automatic analysis with fluid segmentation

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3918907A (en) * 1973-10-29 1975-11-11 Beckman Instruments Inc Micro automatic amino acid analysis process and system
WO1982000773A1 (en) * 1980-09-02 1982-03-18 Chemical Co Dow Liquid chromatographic method and apparatus with hollow fiber device for post-column derivatization
US4451374A (en) * 1980-09-02 1984-05-29 The Dow Chemical Company Liquid chromatographic method and post-column effluent treatment for detection and separation at optimized pH
EP2438938A1 (en) * 2010-10-11 2012-04-11 PharmaSens AG Syringe type pump
WO2012049080A3 (en) * 2010-10-11 2012-06-28 Pharmasens Ag Syringe type pump
CN103313741A (en) * 2010-10-11 2013-09-18 法玛森斯股份公司 Syringe type pump
JP2014502855A (en) * 2010-10-11 2014-02-06 ファルマセンス アクチェンゲゼルシャフト Syringe type pump
CN103313741B (en) * 2010-10-11 2015-07-15 法玛森斯股份公司 Syringe type pump
JP2016190058A (en) * 2010-10-11 2016-11-10 ファルマセンス アクチェンゲゼルシャフト Syringe type pump
US10117989B2 (en) 2010-10-11 2018-11-06 Pharmasens Ag Syringe type pump
US10130756B2 (en) 2010-10-11 2018-11-20 Pharmasens Ag Syringe type pump
CN103619377A (en) * 2011-04-05 2014-03-05 法玛森斯股份公司 Dermally affixed device for intravenous access

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CH447658A (en) 1967-11-30
DE1598254A1 (en) 1971-01-28
GB1096253A (en) 1967-12-20
SE338448B (en) 1971-09-06

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